反应详情

All reaction steps were carried out with protection from light due to the sensitive nature of the azido group. First, a mixture of NaN3 (300 mg, 4.6 mmol) and methyl pentafluorobenzoate (0.972 g, 4.3 mmol) in acetone (8 mL) and water (3 mL) was refluxed for 8 hours. The mixture was cooled, diluted with 10 mL of water, and then extracted with diethyl ether (3×10 mL). The extract was dried (anhydrous Na2SO4) and evaporated to give methyl 4-azido-2,3,5,6-tetrafluorobenzoate (1.01 g, 94%), as off-white flakes, mp 53.6-54.3° C.

1. customAll reaction steps
2. temperaturewas refluxed for 8 hours
3. temperatureThe mixture was cooled
4. extractionextracted with diethyl ether (3×10 mL)
5. dry with materialThe extract was dried (anhydrous Na2SO4)
6. customevaporated